三维铋系光催化剂纳米结构的合成及其光催化性能的调控
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摘要
随着现代工业的快速发展，越来越多的有机污染物进入水环境中，对人类的生存造成严重威胁。相对于传统的处理技术（如吸附法、生物法），光催化氧化技术由于能够有效地去除水体中高稳定性和高毒性的有机污染物，已逐渐成为环境保护领域研究的热点。二氧化钛（TiO_2）具有高效、无毒、稳定及廉价等优点，是光催化领域中应用最为广泛的一种半导体光催化剂，但由于其仅能被紫外光激发而制约了其对太阳光（紫外光仅占太阳光谱的4%）的有效利用，因此，致力于开发新型利用太阳光降解有机污染物的光催化剂具有重要的研究意义。本论文主要研究通过一步简单溶剂热/水热法合成易回收、太阳光响应的三维铋系光催化剂纳米结构，采用各种分析技术对其进行表征，并对其光催化性能进行调控，提高其利用太阳光去除水体中有机污染物的能力。
以五水硝酸铋和偏钒酸铵为原料，采用一步溶剂热法合成高产率、由纳米粒子组装而成的具孔三维花生形貌BiVO_4纳米光催化剂，通过X射线衍射（XRD）、X射线能谱（EDS）、扫描电镜（SEM）、透射电镜（TEM）、紫外-可见漫反射光谱（UV-Vis/DRS）及氮吸附等手段对其成分、结构、尺寸、形貌、光学性质及表面孔结构进行表征，并探讨该三维BiVO_4纳米结构的形成机理。在溶剂热合成条件下，乙二醇对三维花生形貌BiVO_4纳米光催化剂的结构及形貌控制具有至关重要的作用。具孔三维BiVO_4纳米光催化剂和H_2O_2的协同作用能很好地利用太阳光降解水体中的有机污染物罗丹明B，同时探讨了BiVO_4/H_2O_2系统去除水体中罗丹明B的降解机理，研究结果表明羟基自由基和空穴共同氧化降解罗丹明B。此外，对具孔三维BiVO_4纳米光催化剂的稳定性及其循环利用性也进行了研究。
模拟太阳光照射下，研究了银离子（Ag~+）对三维BiVO_4纳米光催化剂降解罗丹明B效果的影响。加入的Ag~+能够有效的捕获BiVO_4导带上的光生电子，从而抑制了光生电子和空穴的复合，提高其光催化降解罗丹明B的活性。理论和实验证实，Ag~+/BiVO_4系统光催化降解罗丹明B主要归结于价带空穴的直接氧化。通过采用X射线衍射（XRD）、透射电镜（TEM）及X射线能谱（EDS）证实Ag~+/BiVO_4系统光催化降解反应后回收得到的三维BiVO_4催化剂表面有金属银纳米颗粒的沉积。光催化降解实验显示沉积在三维BiVO_4催化剂表面的银纳米颗粒又能提高其光催化降解罗丹明B的效果，因此，实验结果证实了加入的Ag~+得到了双重的利用。
以五水硝酸铋和二水钨酸钠为原料，采用一步简单、经济水热法合成由纳米片组装而成的三维Bi_2WO_6微米球，产率高，通过X射线衍射（XRD）、拉曼光谱（Raman）、扫描电镜（SEM）、透射电镜（TEM）、紫外-可见漫反射光谱（UV-Vis/DRS）及氮吸附等分析技术对其结构、形貌、尺寸、光学性质及表面孔结构进行表征。模拟太阳光照射下，三维Bi_2WO_6微米球具有优异的光催化降解罗丹明B的活性。此外，详细阐述了三维Bi_2WO_6微米球光催化降解罗丹明B的机理，证实光生空穴与超氧自由基共同氧化去除罗丹明B。同时实验表明三维Bi_2WO_6微米球在酸性及碱性条件下能够保持稳定，不易转变成其它物质，但在碱性条件下三维Bi_2WO_6微米球降解活性有所降低。在少量H_2O_2的协助下，三维Bi_2WO_6微米球去除高稳定性苯酚的能力大大提升，主要是由于在光照条件下Bi_2WO_6微米球导带上的电子与H_2O_2能够产生强氧化性的羟基自由基，从而导致苯酚的快速降解。
以十六烷基三甲基溴化铵为软模板，五水硝酸铋和二水钨酸钠为原料，采用一步水热法合成三维Bi_2O_3/Bi_2WO_6复合微米球，通过X射线衍射（XRD）、X射线光电子能谱（XPS）、扫描电镜（SEM）、透射电镜（TEM）、紫外-可见漫反射光谱（UV-Vis/DRS）和氮吸附等分析手段对其进行表征。真实太阳光及模拟太阳光照射下，三维Bi_2O_3/Bi_2WO_6复合微米球光催化剂对罗丹明B具有很高的光催化降解活性，活性远高于单独的Bi_2O_3催化剂和Bi_2WO_6催化剂，这主要是由于两者复合时具有合适的能带位置，使电子-空穴对能够有效分离，提高了光利用率。
With the rapid development of modern industry, more and moreorganic pollutants were released into water environment, which posed agreat threat to human survival. Compared with the traditional treatmenttechnology, such as absorption and biological methods, photocatalysisoxidation technology has attracted considerable attention because it canefficiently remove the stable and toxic organic pollutants in water. As awidely used photocatalyst, titania owns some outstanding advantages,such as highly efficient, non-toxic, stable and low-cost. However, titaniais only excited by UV light, which limits its efficient utilization of solarlight because the UV light range accounts for about4%of the solarspectrum. Therefore, it is highly necessary to develop new kinds ofvisible-light-induced photocatalysts using solar light to degrade organicpollutants in water. In this thesis, we mainly focus on design anddevelopment of recyclable sunlight-induced three dimensional (3D) Bi-based photocatalyst nanostructures by one-step facilesolvothermal/hydrothermal route. The as-obtained3D Bi-basedphotocatalyst nanostructures were characterized using various analytictechnologies, and the photocatalytic activities of Bi-based nanostructureswere controlled to enhance their abilities to remove organic pollutants inwater using solar light.
3D porous peanut-shaped BiVO_4nano-photocatalysts assembled bynanoparticles were solvothermally synthesized with high yield byemploying bismuth nitrate and ammonium metavanadate as the startingmaterials. The as-obtained BiVO_4nano-photocatalysts were characterizedby X-ray powder diffraction, energy dispersive spectroscopy, scanningelectron microscopy, transmission electron microscopy, UV-Vis diffusereflectance spectroscopy and nitrogen sorption. The possible formationmechanism of3D peanut-shaped BiVO_4nano-photocatalysts wasdiscussed in detail. In the solvothermal condition, ethylene glycol played an important role in controlling the phase and morphology of theas-synthesized3D peanut-shaped BiVO_4nano-photocatalysts. In theH_2O_2-containing system, the photocatalytic ability of3D peanut-shapedBiVO_4nano-photocatalysts was greatly enhanced to degrade RhB inwater using solar light. The photocatalytic mechanism of porousBiVO_4/H_2O_2/sunlight/RhB system was also proposed, and the resulstsindicated that RhB was oxidized by OH and holes. In addition, thestability and reuse of3D peanut-shaped BiVO_4nano-photocatalysts inthe H_2O_2-containing system were also investigated.
The effect of Ag~+ions for the RhB photodegradation in3D BiVO_4suspension was discussed under simulated solar light irradiation. Thephotoinduced electrons on the conduction band of BiVO_4were capturedby Ag~+ions, which suppressed the recombination of electrons and holes.The theoretical and experimental results indicated that RhB was oxidizedby holes in the Ag~+/BiVO_4system using simulated solar light. X-ray powder diffraction, energy dispersive spectroscopy, and transmissionelectron microscopy confirmed that metal Ag nanoparticles weredeposited on the3D BiVO_4photocatalysts after the photocatalyticreaction. The Ag/BiVO_4composite photocatalysts showed a higherphotocatalytic activity than pure BiVO_4photocatalysts. Obviously, Ag~+ions played the dual role to enhance the photocatalytic ability of3DBiVO_4photocatalysts for RhB degradation.
3D Bi_2WO_6microspheres assembled by nanosheets were preparedwith high yield via one-step simple hydrothermal method, by employingbismuth nitrate and sodium tungstate as the starting materials. Theas-obtained Bi_2WO_6microspheres were characterized by X-ray powderdiffraction, Raman, scanning electron microscopy, transmission electronmicroscopy, UV-Vis diffuse reflectance spectroscopy and nitrogensorption. Under simulated solar light,3D Bi_2WO_6microspheres showedan excellent photocatalytic ability to degrade RhB in water, and the photodegradation mechanism was also proposed. The results indicatedthat RhB was degraded by holes and O–2radicals. The Bi_2WO_6microspheres could keep stable in acid or basic condition, and thephotocatalytic ability would be decrease in basic condition. Thephotocatalytic performance of the Bi_2WO_6microspheres for phenoldegradation was greatly enhanced with the assistance of a small amountof H_2O_2because of more OH radicals produced.
3D Bi_2O_3/Bi_2WO_6composite microspheres were hydrothermallysynthesized by using CTAB as soft template, and bismuth nitrate andsodium tungstate as the starting materials. The as-obtained Bi_2O_3/Bi_2WO_6composite microspheres were characterized by X-ray powder diffraction,X-ray photoelectron spectroscopy, scanning electron microscopy,transmission electron microscopy, UV-Vis diffuse reflectancespectroscopy and nitrogen sorption. Under solar light irradiation,3DBi_2O_3-Bi_2WO_6composite microspheres exhibited a much higher efciency in the photodecomposition of RhB than Bi_2O_3catalyst orBi_2WO_6catalyst. The excellent photocatalytic activity of Bi_2O_3-Bi_2WO_6composite microspheres could be mainly attributed to their strongabsorption in light and low recombination rate of the electrons and holesbecause of the heterojunction formed between Bi_2O_3and Bi_2WO_6.
以五水硝酸铋和偏钒酸铵为原料，采用一步溶剂热法合成高产率、由纳米粒子组装而成的具孔三维花生形貌BiVO_4纳米光催化剂，通过X射线衍射（XRD）、X射线能谱（EDS）、扫描电镜（SEM）、透射电镜（TEM）、紫外-可见漫反射光谱（UV-Vis/DRS）及氮吸附等手段对其成分、结构、尺寸、形貌、光学性质及表面孔结构进行表征，并探讨该三维BiVO_4纳米结构的形成机理。在溶剂热合成条件下，乙二醇对三维花生形貌BiVO_4纳米光催化剂的结构及形貌控制具有至关重要的作用。具孔三维BiVO_4纳米光催化剂和H_2O_2的协同作用能很好地利用太阳光降解水体中的有机污染物罗丹明B，同时探讨了BiVO_4/H_2O_2系统去除水体中罗丹明B的降解机理，研究结果表明羟基自由基和空穴共同氧化降解罗丹明B。此外，对具孔三维BiVO_4纳米光催化剂的稳定性及其循环利用性也进行了研究。
模拟太阳光照射下，研究了银离子（Ag~+）对三维BiVO_4纳米光催化剂降解罗丹明B效果的影响。加入的Ag~+能够有效的捕获BiVO_4导带上的光生电子，从而抑制了光生电子和空穴的复合，提高其光催化降解罗丹明B的活性。理论和实验证实，Ag~+/BiVO_4系统光催化降解罗丹明B主要归结于价带空穴的直接氧化。通过采用X射线衍射（XRD）、透射电镜（TEM）及X射线能谱（EDS）证实Ag~+/BiVO_4系统光催化降解反应后回收得到的三维BiVO_4催化剂表面有金属银纳米颗粒的沉积。光催化降解实验显示沉积在三维BiVO_4催化剂表面的银纳米颗粒又能提高其光催化降解罗丹明B的效果，因此，实验结果证实了加入的Ag~+得到了双重的利用。
以五水硝酸铋和二水钨酸钠为原料，采用一步简单、经济水热法合成由纳米片组装而成的三维Bi_2WO_6微米球，产率高，通过X射线衍射（XRD）、拉曼光谱（Raman）、扫描电镜（SEM）、透射电镜（TEM）、紫外-可见漫反射光谱（UV-Vis/DRS）及氮吸附等分析技术对其结构、形貌、尺寸、光学性质及表面孔结构进行表征。模拟太阳光照射下，三维Bi_2WO_6微米球具有优异的光催化降解罗丹明B的活性。此外，详细阐述了三维Bi_2WO_6微米球光催化降解罗丹明B的机理，证实光生空穴与超氧自由基共同氧化去除罗丹明B。同时实验表明三维Bi_2WO_6微米球在酸性及碱性条件下能够保持稳定，不易转变成其它物质，但在碱性条件下三维Bi_2WO_6微米球降解活性有所降低。在少量H_2O_2的协助下，三维Bi_2WO_6微米球去除高稳定性苯酚的能力大大提升，主要是由于在光照条件下Bi_2WO_6微米球导带上的电子与H_2O_2能够产生强氧化性的羟基自由基，从而导致苯酚的快速降解。
以十六烷基三甲基溴化铵为软模板，五水硝酸铋和二水钨酸钠为原料，采用一步水热法合成三维Bi_2O_3/Bi_2WO_6复合微米球，通过X射线衍射（XRD）、X射线光电子能谱（XPS）、扫描电镜（SEM）、透射电镜（TEM）、紫外-可见漫反射光谱（UV-Vis/DRS）和氮吸附等分析手段对其进行表征。真实太阳光及模拟太阳光照射下，三维Bi_2O_3/Bi_2WO_6复合微米球光催化剂对罗丹明B具有很高的光催化降解活性，活性远高于单独的Bi_2O_3催化剂和Bi_2WO_6催化剂，这主要是由于两者复合时具有合适的能带位置，使电子-空穴对能够有效分离，提高了光利用率。
With the rapid development of modern industry, more and moreorganic pollutants were released into water environment, which posed agreat threat to human survival. Compared with the traditional treatmenttechnology, such as absorption and biological methods, photocatalysisoxidation technology has attracted considerable attention because it canefficiently remove the stable and toxic organic pollutants in water. As awidely used photocatalyst, titania owns some outstanding advantages,such as highly efficient, non-toxic, stable and low-cost. However, titaniais only excited by UV light, which limits its efficient utilization of solarlight because the UV light range accounts for about4%of the solarspectrum. Therefore, it is highly necessary to develop new kinds ofvisible-light-induced photocatalysts using solar light to degrade organicpollutants in water. In this thesis, we mainly focus on design anddevelopment of recyclable sunlight-induced three dimensional (3D) Bi-based photocatalyst nanostructures by one-step facilesolvothermal/hydrothermal route. The as-obtained3D Bi-basedphotocatalyst nanostructures were characterized using various analytictechnologies, and the photocatalytic activities of Bi-based nanostructureswere controlled to enhance their abilities to remove organic pollutants inwater using solar light.
3D porous peanut-shaped BiVO_4nano-photocatalysts assembled bynanoparticles were solvothermally synthesized with high yield byemploying bismuth nitrate and ammonium metavanadate as the startingmaterials. The as-obtained BiVO_4nano-photocatalysts were characterizedby X-ray powder diffraction, energy dispersive spectroscopy, scanningelectron microscopy, transmission electron microscopy, UV-Vis diffusereflectance spectroscopy and nitrogen sorption. The possible formationmechanism of3D peanut-shaped BiVO_4nano-photocatalysts wasdiscussed in detail. In the solvothermal condition, ethylene glycol played an important role in controlling the phase and morphology of theas-synthesized3D peanut-shaped BiVO_4nano-photocatalysts. In theH_2O_2-containing system, the photocatalytic ability of3D peanut-shapedBiVO_4nano-photocatalysts was greatly enhanced to degrade RhB inwater using solar light. The photocatalytic mechanism of porousBiVO_4/H_2O_2/sunlight/RhB system was also proposed, and the resulstsindicated that RhB was oxidized by OH and holes. In addition, thestability and reuse of3D peanut-shaped BiVO_4nano-photocatalysts inthe H_2O_2-containing system were also investigated.
The effect of Ag~+ions for the RhB photodegradation in3D BiVO_4suspension was discussed under simulated solar light irradiation. Thephotoinduced electrons on the conduction band of BiVO_4were capturedby Ag~+ions, which suppressed the recombination of electrons and holes.The theoretical and experimental results indicated that RhB was oxidizedby holes in the Ag~+/BiVO_4system using simulated solar light. X-ray powder diffraction, energy dispersive spectroscopy, and transmissionelectron microscopy confirmed that metal Ag nanoparticles weredeposited on the3D BiVO_4photocatalysts after the photocatalyticreaction. The Ag/BiVO_4composite photocatalysts showed a higherphotocatalytic activity than pure BiVO_4photocatalysts. Obviously, Ag~+ions played the dual role to enhance the photocatalytic ability of3DBiVO_4photocatalysts for RhB degradation.
3D Bi_2WO_6microspheres assembled by nanosheets were preparedwith high yield via one-step simple hydrothermal method, by employingbismuth nitrate and sodium tungstate as the starting materials. Theas-obtained Bi_2WO_6microspheres were characterized by X-ray powderdiffraction, Raman, scanning electron microscopy, transmission electronmicroscopy, UV-Vis diffuse reflectance spectroscopy and nitrogensorption. Under simulated solar light,3D Bi_2WO_6microspheres showedan excellent photocatalytic ability to degrade RhB in water, and the photodegradation mechanism was also proposed. The results indicatedthat RhB was degraded by holes and O–2radicals. The Bi_2WO_6microspheres could keep stable in acid or basic condition, and thephotocatalytic ability would be decrease in basic condition. Thephotocatalytic performance of the Bi_2WO_6microspheres for phenoldegradation was greatly enhanced with the assistance of a small amountof H_2O_2because of more OH radicals produced.
3D Bi_2O_3/Bi_2WO_6composite microspheres were hydrothermallysynthesized by using CTAB as soft template, and bismuth nitrate andsodium tungstate as the starting materials. The as-obtained Bi_2O_3/Bi_2WO_6composite microspheres were characterized by X-ray powder diffraction,X-ray photoelectron spectroscopy, scanning electron microscopy,transmission electron microscopy, UV-Vis diffuse reflectancespectroscopy and nitrogen sorption. Under solar light irradiation,3DBi_2O_3-Bi_2WO_6composite microspheres exhibited a much higher efciency in the photodecomposition of RhB than Bi_2O_3catalyst orBi_2WO_6catalyst. The excellent photocatalytic activity of Bi_2O_3-Bi_2WO_6composite microspheres could be mainly attributed to their strongabsorption in light and low recombination rate of the electrons and holesbecause of the heterojunction formed between Bi_2O_3and Bi_2WO_6.
引文
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